Method for preparing arctiin

A technique for arctiside and arctium seed, which is applied in the field of preparation of arctiside, can solve the problems of purification treatment, influence on purity and yield, many impurities, low purity and the like, and achieves easy industrial production, high yield and no environment. The effect of pollution

Active Publication Date: 2012-02-15
SHANGHAI HUIWEN BIO TECH
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  • Application Information

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Problems solved by technology

However, because the hot reflux extract of arctiin is very turbid and has many impurities, it is generally treated with organic solvent degreasing or clarifying agent; at the same time, because arctiin contains a lactone ring structure, it is easily hydrolyzed under heating conditions. Negative impact on purity and yield
The general product purity of the existing process is lower than 70%, and the yield of the recrystallization technology is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 200 grams of burdock fruit medicinal material, ultrasonically extracted twice (10 times, 10 times) by 20 times of water, each time for 1 hour, the extract was left to stand, filtered, the filtrates were combined, put on D101 column (column volume 300ml / BV), and loaded Then use 2BV water, 2BV 30% ethanol, 3BV 75% ethanol to elute successively, collect the 70% ethanol eluted part, concentrate, add water to dilute the concentrate to 200ml, put it on LSA-700 resin column (column volume 200ml / BV), put it on After the sample was eluted with 2BV of water and 2BV of 60% ethanol in turn, the 60% ethanol eluate was collected, concentrated to 50ml, added 2% polyamide at room temperature and stirred for 30min, filtered, and the filtrate was added with 1 times the amount of acetone at 0~5℃ Crystallized overnight, filtered, and dried to obtain 5.17 g of arctiin, with a purity of 96.3% detected by HPLC according to Part 1 of the Chinese Pharmacopoeia 2010 edition.

Embodiment 2

[0021] 200 grams of burdock fruit medicinal material, extracted twice by 30 times of water (15 times, 15 times), each time for 2 hours, the extract was left to stand, filtered, the filtrates were combined, put on the LX38 column (column volume 300ml / BV), and loaded Then use 2BV water, 2BV 10% ethanol, 3BV 40% ethanol to elute successively, collect the 40% ethanol eluted part, concentrate, add water to dilute the concentrated solution to 200ml, put on DDW-16 resin column (column volume 200ml / BV), put on After the sample was eluted successively with 2BV of water and 2BV of 60% ethanol, the 60% ethanol eluate was collected, concentrated to 50ml, filtered, and 2 times the amount of ethanol was added to the filtrate to crystallize overnight at 0-5°C, filtered, and dried to obtain Arctium Glycoside 5.79g, purity 95.8%.

Embodiment 3

[0023] 200 grams of burdock fruit medicinal material, extracted by microwave heating twice (20 times, 20 times) with 40 times of water, each time for 1 hour, the extract was left to stand, filtered, the filtrates were combined, and put on the AB-8 column (column volume 300ml / BV) , eluted with 2BV water, 2BV 25% ethanol, and 3BV 60% ethanol successively after loading the sample, collected the 60% ethanol eluted part, concentrated, and the concentrated solution was diluted to 200ml with water, and put on a D-318 resin column (column volume 200ml / BV ), followed by elution with 2BV of water and 2BV of 50% ethanol after loading the sample, collecting the 50% ethanol eluate, concentrating to 50ml, adding 0.5% activated carbon to boil for 30min, filtering, adding 1 times the amount of methanol to the filtrate at 0~5℃ Crystallized overnight, filtered, and dried to obtain 4.98 g of arctiin with a purity of 98.7%.

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Abstract

The invention discloses a method for preparing arctiin. The method mainly comprises the following steps of: extracting a burdock medicinal material with water; filtering the extracting solution, and directly introducing into a macroporous resin column for adsorbing and enriching; eluting gradually with water and an ethanol solution in sequence; collecting the needed eluent, concentrating and filtering; treating with a decoloring resin column to obtain crude arctiin; and crystallizing with a water-containing mixed solvent to obtain a finished product of which the purity is more than 90 percent. The method has the advantages of simple process, continuous operation, convenience in automation, convenience for recycling solvents, low energy consumption, high product purity and easiness for realizing industrial amplification.

Description

technical field [0001] The invention relates to a preparation method of arctiin. technical background [0002] Burdock Fructus is the dry and mature fruit of Arctium burdock, a plant of Compositae. It is mainly used to treat diseases such as wind-heat cold, measles, carbuncle and sore, and is a traditional Chinese medicine in my country. Arctium contains lignin compounds whose main component is arctiin. Modern pharmacological studies have shown that Burdock Fructus has pharmacological effects such as antibacterial, anti-tumor, anti-nephropathy, enhancing the body's immune function, anti-hypertension, and hypoglycemia. Arctiin and its oral transformation component arctigenin are its main active ingredients, which can be used in the fields of related medicines and functional foods. See Wang Lu et al. "Research Progress on the Pharmacological Actions of Arctiin and Arctigenin" (Chinese Herbal Medicine, 2008: 467-470.) and related literature. [0003] In recent years, the ind...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/26C07H1/08
Inventor 刘江云彭晓国何钦王国丽梁斌李孟林唐靖雯
Owner SHANGHAI HUIWEN BIO TECH
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